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The carbon black-oxide (CBO) particles were prepared by oxidizing carbon black (CB) in a modified Hummer's method to improve the dispersion of CBO in water. The carboxylic acid, epoxide groups, and hydroxyl groups were formed in the resulting golden CBO particles, which in the size of about 30−50 nm were smaller than CB particles. And the dispersion of CBO particles was so good in distilled water that CBO particles in aqueous solution followed the Lambert−Beer's law well. The nanocomposites were also prepared using CBO or CB particles as the fillers in glycerol-plasticized starch (GPS) matrix by the casting process. CBO fillers had good dispersion in GPS matrix and exhibited an obvious reinforcing effect. Both tensile strength and Youngs modulous of GPS/CBO composites were higher than GPS/CB composites. In views of the values of water vapor permeability (WVP), GPS/CBO composites exhibited better water resistance than GPS/CB composites.